CN105819469B - 一种利用高温催化氧化处理双甘膦废盐的方法 - Google Patents
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Abstract
本发明公开了一种利用高温催化氧化处理双甘膦废盐的方法,涉及废盐处理技术领域,包括如下步骤:(1)除渣,(2)高温催化氧化,(3)除磷,(4)纯化。本发明利用双甘膦在230℃时开始熔融并分解,将盐渣置于热分解炉内,在高温条件下,双甘膦等有机物氧化分解,氮以气体形势挥发出去,达到与盐渣分离的目的;有机磷则在高温条件下转化成无机磷存在于固体盐中,将热分解后的盐用水溶解,然后用除磷剂其中的磷沉淀下来,经过滤和纯化得到符合要求的工业原料盐。
Description
技术领域:
本发明涉及废盐处理技术领域,具体涉及一种利用高温催化氧化处理双甘膦废盐的方法。
背景技术:
生产农药时,通常会通过加入盐酸进行中和,中和后会产生大量的副产品废盐,其中氯化钠含量达到70%以上,同时含有大量的有机或无机杂质。双甘膦盐渣中除了含有大量氯化钠外,还含有少量的亚磷酸钠、双甘膦、甲醛等有害杂质,不能直接用作工业原料盐。为了降低对环境的污染,实现资源的合理回收利用,本公司开发出一种利用高温催化氧化处理双甘膦废盐的方法,通过高温催化氧化除去废盐中的有害物质,最终处理后得到的产物可直接用作工业原料盐。
发明内容:
本发明所要解决的技术问题在于提供一种处理效率高、成本低的利用高温催化氧化处理双甘膦废盐的方法。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种利用高温催化氧化处理双甘膦废盐的方法,包括如下步骤:
(1)除渣:将双甘膦废盐加入水中,浸泡24h后机械搅拌,待固体基本溶解完全后加入固体吸附剂,搅拌混合12h,过滤,滤液经浓缩成膏体后送入冷冻干燥机,所得固体再经粉碎机制成粗盐,然后将粗盐置于干燥环境下堆放24-48h,保持空气流通;
(2)高温催化氧化:向上述所得粗盐中加入催化剂,充分混合后置于分解炉中,先加热至100-110℃保温10-15min,再加热至230-240℃保温15-30min,然后继续加热至320-330℃保温30-45min;
(3)除磷:将上述经高温催化氧化后的粗盐加入水中,完全溶解后过滤,向滤液中加入除磷剂,搅拌3-5h后静置过夜,再次过滤,收集滤液;
(4)纯化:将上述所得滤液蒸发浓缩至含水量低于30%,然后置于0-5℃下自然析晶,最后离心过滤,即得工业原料盐。
所述固体吸附剂由如下重量百分比的原料组成:凹凸棒土30%、聚合氯化铁15%、明矾12%、聚合硅酸铝12%、活性炭10%、氢氧化镁8%、木质素磺酸钠8%、焦亚硫酸钠5%。
所述催化剂由重量百分比为80%主催化剂和20%助催化剂组成,主催化剂是以氧化铝为载体、五氧化二钒为活性组分在惰性环境中于120-130℃下研磨1h制成的,助催化剂选自硫酸钾和硫酸钠中的一种或混合物。
所述除磷剂由如下重量百分比的原料组成:石膏粉45%、聚合硫酸铝15%、聚丙烯酰胺12%、聚丙烯酸钠10%、柠檬酸钙8%、偏硅酸钙5%、尿素4%、硼砂1%。
本发明的有益效果是:本发明利用双甘膦在230℃时开始熔融并分解,将盐渣置于热分解炉内,在高温条件下,双甘膦等有机物氧化分解,氮以气体形势挥发出去,达到与盐渣分离的目的;有机磷则在高温条件下转化成无机磷存在于固体盐中,将热分解后的盐用水溶解,然后用除磷剂其中的磷沉淀下来,经过滤和纯化得到符合要求的工业原料盐。
具体实施方式:
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
一种利用高温催化氧化处理双甘膦废盐的方法,包括如下步骤:
(1)除渣:将双甘膦废盐加入水中,浸泡24h后机械搅拌,待固体基本溶解完全后加入固体吸附剂,搅拌混合12h,过滤,滤液经浓缩成膏体后送入冷冻干燥机,所得固体再经粉碎机制成粗盐,然后将粗盐置于干燥环境下堆放24h,保持空气流通;
(2)高温催化氧化:向上述所得粗盐中加入催化剂,充分混合后置于分解炉中,先加热至100-110℃保温10min,再加热至230-240℃保温25min,然后继续加热至320-330℃保温30min;
(3)除磷:将上述经高温催化氧化后的粗盐加入水中,完全溶解后过滤,向滤液中加入除磷剂,搅拌3h后静置过夜,再次过滤,收集滤液;
(4)纯化:将上述所得滤液蒸发浓缩至含水量低于30%,然后置于0-5℃下自然析晶,最后离心过滤,即得工业原料盐。
固体吸附剂由如下重量百分比的原料组成:凹凸棒土30%、聚合氯化铁15%、明矾12%、聚合硅酸铝12%、活性炭10%、氢氧化镁8%、木质素磺酸钠8%、焦亚硫酸钠5%。
催化剂由重量百分比为80%主催化剂和20%助催化剂组成,主催化剂是以氧化铝为载体、五氧化二钒为活性组分在惰性环境中于120-130℃下研磨1h制成的,助催化剂选自硫酸钾和硫酸钠中的一种或混合物。
除磷剂由如下重量百分比的原料组成:石膏粉45%、聚合硫酸铝15%、聚丙烯酰胺12%、聚丙烯酸钠10%、柠檬酸钙8%、偏硅酸钙5%、尿素4%、硼砂1%。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (1)
1.一种利用高温催化氧化处理双甘膦废盐的方法,其特征在于,包括如下步骤:
(1) 除渣:将双甘膦废盐加入水中,浸泡24 h后机械搅拌,待固体溶解完全后加入固体吸附剂,搅拌混合12 h,过滤,滤液经浓缩成膏体后送入冷冻干燥机,所得固体再经粉碎机制成粗盐,然后将粗盐置于干燥环境下堆放24-48 h,保持空气流通;
(2) 高温催化氧化:向上述所得粗盐中加入催化剂,充分混合后置于分解炉中,先加热至100-110℃保温10-15 min,再加热至230-240℃保温15-30 min,然后继续加热至320-330℃保温30-45 min;
(3) 除磷:将上述经高温催化氧化后的粗盐加入水中,完全溶解后过滤,向滤液中加入除磷剂,搅拌3-5 h后静置过夜,再次过滤,收集滤液;
(4) 纯化:将上述所得滤液蒸发浓缩至含水量低于30%,然后置于0-5℃下自然析晶,最后离心过滤,即得工业原料盐;
所述固体吸附剂由如下重量百分比的原料组成:凹凸棒土 30%、聚合氯化铁 15%、明矾12%、聚合硅酸铝12%、活性炭 10%、氢氧化镁 8%、木质素磺酸钠 8%、焦亚硫酸钠 5%;
所述催化剂由重量百分比为80%主催化剂和 20%助催化剂组成,主催化剂是以氧化铝为载体、五氧化二钒为活性组分在惰性环境中于120-130℃下研磨1 h制成的,助催化剂选自硫酸钾和硫酸钠中的一种或其混合物;
所述除磷剂由如下重量百分比的原料组成:石膏粉 45%、聚合硫酸铝 15%、聚丙烯酰胺12%、聚丙烯酸钠 10%、柠檬酸钙 8%、偏硅酸钙 5%、尿素 4%、硼砂 1%。
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